北京市蔬菜、水果中有机磷农药残留现状调查

为了解北京市蔬菜、水果中有机磷农药残留情况,2002年在北京市抽检样品354件进行13种有机磷监测,其中蔬菜28l件,水果73件。检测结果显示7．6％的检品不符合国家标准。叶菜类(14,占9．3％)和根茎类(8,占17．4％)蔬菜的不合格率明显高于瓜菜、果菜类(2,占2．4％)蔬菜和水果(3,占4．1％)。13种有机磷检测出12种,其中禁用农药占53％。本市种植的蔬菜、水果与外埠进京产品的有机磷农药残留情况无显差别,超市、集贸市场、批发市场销售的产品的不合格率亦无显差别。     

澳门地区市售叶类菜有机磷农药残留检测:2000～2003

目的了解澳门地区叶类菜残留有机磷农药的情况。方法2000年至2003年间分别于澳门各菜市场、街头摊贩、蔬果杂货店等地点抽取了共817件叶类菜样本,以检测有机磷农药残留水平。结果2000年至2003年度,叶类菜残留有机磷农药不合格率平均为73%、132%、131%、149%,历年不合格率呈上升趋势(AdjustedR2=0074,P=003)。除2002年外,每年从街头摊贩所取得样本之不合格率均比从菜市场所抽取者为高,且差异具统计学意义(P<005)。构成历年不合格样本的原因,主要是甲胺磷和马拉硫磷农药残留超逾标准所致;各类叶类菜样本中亦以通心菜样本中残留有机磷农药的检出之不合格率最高,约占通心菜样本总数四成。讨论考虑到“农场到餐桌”食物链的全过程,除了农场方面对农药的正确和安全使用需要回顾外,农药的生产管理,以至营销流通监管亦不能掉以轻心,政府和有关部门必须高度重视。     

蔬菜中有机磷和氨基甲酸酯类农药残留量的快速检测方法研究

为快速检测蔬菜上的农药残留,建立了两种快速检测方法,速测卡法和酶抑制率法,速测卡法和酶抑制率法对农药的检出限,根据农药的不同而有所不同,速测卡法的检出限一般在0．3－3.5mg/kg,酶抑制率法一般在0．05－5．0mg/kg,速测卡法的检出时间为15min,酶抑制率法的检出时间为30min,两种方法可用于现场检测,操作简单,速度快,测试成本低廉,对超对我国国家标准允许留限量或违禁使用的有机磷和氨基甲酸酯类农药的有效检出率可80%上,两种方法适合我国蔬菜中部分农药残留量的监督检测。     

近红外光谱法（NIR）快速诊断蔬菜中有机磷农药残留

本文首次采用傅立叶变换近红外光谱法(FT—NIR)对十字花科、旋药科、菊科、伞形花科、苋科等二十余种叶菜类中有机磷农药残留的鉴别进行了系统研究，以农药甲胺磷为主要研究对象，结合其他三种高、中、低毒有机磷类进行分析测试，讨论了各种蔬菜样品谱图的差异，利用含磷基团在倍频区的特征吸收，采用差谱技术、导数预处理等进行指认，与GC—MS法比对，取得满意的鉴别效果，为有机磷农药残留的快速分析提供一种简便、快速、可靠的手段。     

蔬菜中有机磷农药残留降解方法的研究进展

目前有机磷农药是应用最为广泛的化学农药之一,蔬菜是其主要作用对象,有机磷农药带来的药残严重威胁人类的健康。对于有机磷药残的降解方法主要有物理降解、化学降解和生物降解,其中生物降解法是应用前景最为广泛的降解方法之一。     

纺织品中有机磷农药残留量检测方法的研究

纺织品及其材料试样经乙酸乙酯超声波提取，提取液浓缩定容后，用配有火焰光度检测器的气相色谱仪（GC—FPD）测定，外标法定量；或用气相色谱-质谱（GC—MS）测定和确证，外标法定量。     

4种叶菜有机磷和氨基甲酸酯类农药残留变化研究

研究了喷施氧化乐果、抗蚜威、敌百虫、敌敌畏对油麦菜、茼蒿、木耳菜、上海青4种叶菜中有机磷和氨基甲酸酯类农药残留的影响及降解变化.结果表明:分别用质量分数90%的晶体敌百虫135 mg/m2,体积分数40%的氧化乐果700倍液喷施4种叶类蔬菜后,其安全间隔期为3 d;用质量分数20%的粉剂抗蚜威135 mg/m2喷施4种蔬菜后,油麦菜、木耳菜、上海青的安全间隔期为3 d,茼蒿的安全间隔期为4 d;用体积分数80%的敌敌畏500倍液喷施,4种叶菜安全间隔期为4 d.     

蔬菜中多种有机磷农药残留气相色谱分析法

为了同时测定蔬菜中13种有机磷农药残留,利用毛细管色谱仪附火焰光度检测器进行检测.蔬菜匀浆后经乙腈提取、净化后,采用程序升温和恒流的方式进行气相色谱分析.结果表明,13种有机磷农药在22.5 min内得到很好分离.有机磷农药残留量在2～1 000 μg/kg范围内线性良好,相关系数为0.998 6～0.999 7.13种混合农药加标浓度为0.1 mg/kg时,平均回收率在73.20 %～101.23 %之间,相对标准偏差小于5 %,检出限0.01～0.05 mg/kg.该方法能一次完成蔬菜中13种有机磷农药残留的分离和测定,操作简便、灵敏.     

Results from the monitoring of pesticide residues in fruit and vegetables on the Danish market, 1998?99

The objective of the Danish pesticide monitoring programme for fruit and vegetables was to check for compliance with the maximum residue levels in foods and to monitor the residue levels to assess the pesticide exposure of the Danish population. Sampling plans were designed based on previous findings and on food consumption data. Approximately 60% of the samples were selected on the basis of positive findings in samples from the previous 5 years. The remaining samples reflected the pattern of food consumption in Denmark. In addition, a rolling programme is maintained for commodities with a low consumption and no detected residues. Within each commodity, the sampling was random. Samples (n = 4150) of mainly fresh, conventionally grown fruit and vegetables were taken throughout the chain of suppliers including foodprocessing companies. Of the samples, 3% were frozen products and 2% were organically grown. Of the samples, 35% were of Danish origin, with 65% originating from other countries. Three accredited laboratories performed analyses of the samples using capillary gas chromatography, liquid chromatography and spectrophotometric methods. Results were registered online into a central database. Residues were found in 54% of the samples of fruit but only in 13% of the vegetables. Residues above the MRL were found in 4% of all samples of fruit and in 1% of vegetables.     

Results from the monitoring of pesticide residues in fruit and vegetables on the Danish market, 2000-01

To check compliance with the maximum residue levels in foods and to monitor the residue levels to enable an evaluation of the exposure of the Danish population to pesticides, a monitoring programme for pesticides residues in fruit and vegetables was performed. Sampling plans were designed based on previous findings and on consumption data. Samples (n = 4404) of mainly fresh conventionally and organically grown fruit and vegetables were collected at wholesalers and importers and at food processing companies. Of the samples, 3% were frozen products and 5% organically grown. Of the samples, 34% were of Danish origin, with 66% from other countries. Two accredited laboratories performed analyses of the samples using capillary gas chromatography, liquid chromatography and a spectrophotometric method. Reporting levels were set at the lowest calibration level or at the limit of determination. Residues were found in 60% of the samples of fruit but in only 18% of the vegetable samples. Residues above the maximum residue levels were found in 6% of all samples of fruit and in 2% of the vegetable samples.     

天津地区果蔬农药施用状况的调查

目的调查天津农民在种植水果蔬菜过程中的农药施用状况。方法对全年随机抽取的3360名农户进行问卷调查,内容涉及施用农药的种类、频次、施药间隔及安全间隔期等。结果2005年天津市施用于水果、蔬菜的农药种类共计140种,以有机磷类杀虫剂为主,占20．7％;按施药频次排序,前10位主要为低毒低残留农药,其中有机磷类杀虫剂一遍净（吡虫啉）施用频次最多,占全年总频次的15．3％;全年总违规施药率为1．59％,四季农药违规施用率差异有统计学意义（P〈0,01）,第三季度违规施用率最高,为2．57％;部分调查果蔬中施药次数违规率较高．其中苹果中氰戊菊酯的施药次数违规率高达95．8％。结论国家明令禁止的农药违规施用率明显好转,但部分农药的施药次数及安全间隔期违规现象比较严重。     

Monitoring of pesticide residues in Egyptian fruits and vegetables during 1997

A total of 2318 domestic samples of different types of fruits and vegetables were collected from eight Egyptian local markets in six different regions of the country. All samples were examined for residues of 54 pesticides, including organophosphorus, organonitrogen, organohalogen and certain pyrethroides. However, dithiocarbamates were analysed in only 318 samples. Overall, 81.5% of the samples had no detectable pesticide residues. Of the contaminated samples, 18.5% contained detectable residues and 1.9% exceeded their maximum residue limits (MRLs). Root and leafy vegetables showed the lowest contamination rates (1.9 and 4.7%, respectively), slightly exceeding the MRLs in leafy vegetables. However, fruit samples showed a slightly higher proportion of contamination than vegetables (29 and 14.3%, respectively). Fruit also exhibited a higher level of violation than vegetables (2.3 and 1.9%, respectively). The contamination and violation rates were lower than the percentages recorded in previous years' monitoring studies. Dicofol and dimethoate were the most frequently occurring pesticide residues at 5.1 and 5.0%, respectively. Dimethoate showed higher violation levels (0.69%). However, dicofol showed a slight violation rate (0.09%) which indicates good agricultural practices for dicofol use. Dithiocarbamates residues were found in 21 of the 318 samples analysed, which when expressed as a percentage contamination was 6.6%, and only one sample exceeded the MRL.     

陕西省2004-2005年蔬菜、水果中农药残留污染状况调查

目的了解陕西地区蔬菜、水果中使用农药残留情况。方法2004年9月和2005年9月对全省6个市县各大农贸市场及超市销售的蔬菜、水果以及个别蔬菜、水果产地的蔬菜、水果随机抽样检查,采用气相色谱仪法及气相色谱-质谱仪法对18种蔬菜、水果中的有机磷、氨基甲酸酯、菊酯、三氯杀螨醇4类22种农药残留量进行测定。结果2年共抽检蔬菜、水果样品455份。2004年采集174份,其中有机磷类农药总检出率18.39%,超标率18.39%。氨基甲酸酯类农药检出率为12.64%,超标率2.87%。菊酯类农药的总检出率为31.03%,均未超标。三氯杀螨醇农药检出率为4.02%,均未超标。2005年采集281份,其中有机磷农药总检出率34.16%,超标率27.40%。氨基甲酸酯类农药检出率5.34%,均未超标。菊酯类农药检出率为52.67%,超标率1.07%。三氯杀螨醇农药检出率为37.01%,超标率6.41%。结论陕西地区蔬菜、水果中滥施农药特别是有机磷和三氯杀螨醇等高毒、剧毒农药的情况较为严重,应加强监督管理。     

叶菜中有机磷农药多组分残留的快速分析

为提高蔬菜中有机磷农药的检测水平,建立了新鲜叶菜样品中37种有机磷农药残留的分析方法。对试样用乙腈一次性提取,凝胶色谱柱净化预处理,毛细管气相色谱法分离,火焰光度检测器的磷滤光片(FPD(P))检测,外标法定量。该方法分离效果良好,重现性好,灵敏度、精密度高,杂质干扰少。所检测的37种有机磷农药的最低检出量在3.36×10-11(甲胺磷)～5.652×10-10g(磷胺)之间,当青菜试样中有机磷农药的添加浓度为0.05～2.0mgkg时,方法回收率在54.57%～112.64%之间。最低检测限和方法添加回收率均符合农药残留分析的要求。本方法操作简便,重现性好,杂质干扰少,测定结果可靠,灵敏度高,无论是进行多组分有机磷快速定量检测,或是突发性有机磷中毒检测均具有较好的适用性。     

固相萃取-高效液相色谱-串联质谱法同时测定水生蔬菜中的5种农药残留

目的 建立固体萃取-高效液相色谱-串联质谱法测定水生蔬菜中甲基对硫磷、灭草松、莠去津、呋喃丹和2,4-滴的分析方法。方法 待测样品均质后加入0.2%甲酸乙腈、氯化钠溶液超声提取30 min,经C18固相萃柱净化后,使用Waters UPLC HSS T3色谱柱进行分离,流动相为0.1%甲酸水溶液-甲醇溶液,以电喷雾离子源ESI（+/-）采用多离子反应监测模式检测。结果 甲基对硫磷、莠去津、呋喃丹和2,4-滴在0.5～20.0 μg/kg、灭草松在0.5～10.0 μg/kg的浓度范围内具有良好的线性关系,相关系数达到了0.99。方法检出限在0.030～0.170 μg/kg之间,方法定量限为0.10～0.50μg/kg。6个不同加标水平的平均加标回收率在86.4%～110.3%,相对标准偏差为0.87%～8.34%。结论 本研究建立的方法简便,准确度高、精密度好,重现性强,适用于同时测定水生蔬菜中甲基对硫磷、灭草松、莠去津、呋喃丹和2,4-滴的5种农药残留量。     

使用微量化学法测定茶叶中有机磷农药残留量的研究

为解决进出口茶叶样品量大, 现有分析方法繁琐, 并且应对欧盟2008年9月后提出的新农药残留限量要求的难题, 本文采用微量化学法, 对分析实验过程中的物料进行逐项缩减, 建立了茶叶中20种有机磷农药多残留检测新方法.茶叶样品经乙酸乙酯-正己烷混合提取, 固相萃取小柱净化, 气相色谱测定.20种有机磷农药标准曲线相关系数(r2)大于0.9990(浓度范围0.010～2.0 mg/L).该方法20种有机磷农药检出限为0.01～0.04 mg/kg.红茶和绿茶不同发酵方法的样品中在0.02～1.0 μg/kg添加范围, 回收率均在60%～120%, 精密度为0.3%～10.2%.